CN106044787B - A kind of preparation method of aeroge - Google Patents
A kind of preparation method of aeroge Download PDFInfo
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- CN106044787B CN106044787B CN201610662434.7A CN201610662434A CN106044787B CN 106044787 B CN106044787 B CN 106044787B CN 201610662434 A CN201610662434 A CN 201610662434A CN 106044787 B CN106044787 B CN 106044787B
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- acid
- solution
- aeroge
- surface area
- specific surface
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to a kind of preparation method of aeroge, which solve existing macro porous silica gel aperture it is not big enough the technical issues of, include the following steps：(1) by aeroge raw material, through extraordinary solution treatment for the first time；(2) first hypo acids steep；(3) second of extraordinary solution treatment；(4) second hypo acids steep；(5) it is dried, obtains aerogel products, extraordinary solution is methanol, one kind in ethylene glycol, glycerine.It the method can be widely used in the preparation field of aeroge.
Description
Technical field
The present invention relates to silicon chemical field, specifically a kind of preparation method of aeroge.
Background technology
Silica gel is generally divided into Kiselgel A, silochrom, macro porous silica gel by its aperture difference in the prior art.Existing skill
Its physical and chemical performance of the macro porous silica gel of art is：Average pore size exists：10~45mm, 250~350 ㎡ of average specific surface area/ɡ, average hole
Hold：1.00~2.00mL/ ɡ.
Current above-described macro porous silica gel index much can not meet the various needs of active user, particularly all kinds of
The application of catalyst and carrier, biochemistry product, natural products isolate and purify, medicine preparation, Separation of Organic Compounds etc.
The application of every field is both needed to the silica gel that the especially big hole of high-specific surface area holds aperture.
Invention content
The present invention be exactly in order to solve the technical issues of existing macro porous silica gel aperture is not big enough, provide a kind of especially big Kong Rong,
Aperture, high-specific surface area aeroge preparation method.
For this purpose, the preparation method of aeroge provided by the invention, includes the following steps：By raw material through 50~90 DEG C of temperature
Expanding treatment makes Kong Rong reach 0.7~0.8ml/g, 5.0~7.0nm of aperture, and specific surface area controlled 550~
650m2/ g reuses extraordinary solution first time immersion treatment, and this solvent can make its strong reaming again, and processing 0.5~72 is small
When after carry out for the first time acid bubble：It is impregnated 5~15 hours in the acid solution for being 0.1~2.5% in content, it is therefore an objective to improve control ratio
Surface area, then with extraordinary second of immersion treatment of solution 0.5~36 hour with reaming again；Then quadratic acid steeps again, in content
To be impregnated again in 0.2~1.5% acid solution 10~20 hours, to improve control specific surface area, so as to obtain product；It is described
Extraordinary solution is methanol, one kind in ethylene glycol, glycerine；Preferably, the mass percent concentration of extraordinary solution is 95%.Acid
Bubble processing acid used is sulfuric acid, one kind in nitric acid, hydrochloric acid, acetic acid, formic acid.
The advantage of the invention is that：There is following pore structure with the BXDK aeroges that this method produces：Average pore size exists
20~55mm, average hole hold 2.2~3.3mL/ ɡ, and specific surface area is in 550~650mL/ ɡ；And there is certain mechanical strength,
Meet the characteristic that water is not split.
Since the raw material that uses of aeroge of the present invention is the raw material of speciality, the inherently high temperature reaming of this raw material,
And specific surface area is increased to the range of requirement and is controlled.This has laid the pore structure of the aeroge of the present invention solid
Basis.Since extraordinary solution used in the present invention impregnates, and this solvent has kind of a unique consumingly reaming effect, due to
The present invention impregnates again through acid adding twice, it is therefore an objective to specific surface area be controlled no longer to reduce.Therefore, aeroge of the invention is due to hole
Hold, aperture it is especially big, specific surface area is extra-high, nanostructured adsorption, inorganic so especially suitable for multiple catalysts and pharmaceutical carrier
Absorption, resin and chromatography；Hydrophilic or hydrophobic etc..
Specific embodiment
According to following embodiments, the present invention may be better understood.It is however, as it will be easily appreciated by one skilled in the art that real
It applies the described content of example and is merely to illustrate the present invention, without this hair described in claims should will not be limited
It is bright.In following embodiment, if without special mark, concentration is mass percent concentration.
Embodiment 1
The BXDK aeroge manufacturing methods of the present invention are using a kind of special BXDK aeroge raw materials, and this raw material is in itself
Just 50~90 DEG C of temperature expanding treatments, make Kong Rong reach 0.7~0.8ml/g, 5.0~7.0nm of aperture, and specific surface area
It has controlled in 550~650m2/ g, reuses a kind of extraordinary solution first time immersion treatment, and this solvent can make it strong again
Reaming, processing carry out acid bubble for the first time after 0.5~72 hour：It is small that 5~15 are impregnated in the acid solution for being 0.1~2.5% in content
When, it is therefore an objective to improve control specific surface area, then with special type solution second of immersion treatment 0.5~36 hour with reaming again；So
Quadratic acid steeps again afterwards, is impregnated again 10~20 hours in the acid solution for being 0.2~1.5% in content, to improve control specific surface
Product, so as to obtain BXDK aerogel products.Specific embodiment is shown in Table 1.
Embodiment 2-6
The step of embodiment 2-6, is same as Example 1, and specific parameter is as shown in table 1.
Table 1：Aeroge manufacturing method technological condition embodiment and its pore structure
The product is especially suitable for multiple catalysts and pharmaceutical carrier, nanostructured adsorption, inorganic adsorbent resin and chromatography,
Hydrophilic or hydrophobic etc..
Claims (1)
1. a kind of preparation method of aeroge, it is characterized in that including the following steps：By raw material through 50~90 DEG C of temperature expanding treatments,
Kong Rong is made to reach 0.7~0.8ml/g, 5.0~7.0nm of aperture, and specific surface area has been controlled in 550~650m2/ g, reuses
Extraordinary solution first time immersion treatment, this solvent can make its strong reaming again, and processing carries out for the first time after 0.5~72 hour
Acid bubble：Is impregnated 5~15 hours in the acid solution for being 0.1~2.5% in content, it is therefore an objective to improve control specific surface area, then with special
Second of immersion treatment of solution is planted 0.5~36 hour with reaming again；Then quadratic acid steeps again, is in mass percent concentration
It is impregnated again in 0.2~1.5% acid solution 10~20 hours, to improve control specific surface area, so as to obtain product；The spy
Kind solution is methanol, one kind in ethylene glycol, glycerine；The mass percent concentration of the special type solution is 95%；The acid
Bubble processing acid used is sulfuric acid, one kind in nitric acid, hydrochloric acid, acetic acid, formic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610662434.7A CN106044787B (en) | 2016-08-12 | 2016-08-12 | A kind of preparation method of aeroge |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610662434.7A CN106044787B (en) | 2016-08-12 | 2016-08-12 | A kind of preparation method of aeroge |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106044787A CN106044787A (en) | 2016-10-26 |
| CN106044787B true CN106044787B (en) | 2018-06-12 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610662434.7A Active CN106044787B (en) | 2016-08-12 | 2016-08-12 | A kind of preparation method of aeroge |
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| CN (1) | CN106044787B (en) |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100376480C (en) * | 2003-02-21 | 2008-03-26 | 青岛海洋化工有限公司 | Production of macroporous silica gel |
| KR101187568B1 (en) * | 2010-09-29 | 2012-10-04 | 한국에너지기술연구원 | Preparation method of silica aerogel granules |
| CN103880024B (en) * | 2012-12-21 | 2015-11-18 | 青岛美格斯科技有限公司 | A kind of preparation method of large pore volume silica-gel carrier |
| CN103043673B (en) * | 2013-01-15 | 2015-11-25 | 北京博天子睿科技有限公司 | A kind of preparation method of aerosil |
| CN103833041B (en) * | 2014-03-04 | 2016-08-17 | 中国科学技术大学 | A kind of constant pressure and dry prepares the method for flexible silica aerogel block |
| CN104876226B (en) * | 2015-05-11 | 2017-11-07 | 爱彼爱和新材料有限公司 | A kind of method for quickly preparing Hydrophobic silica aeroge with the subcritical drying of methanol |
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2016
- 2016-08-12 CN CN201610662434.7A patent/CN106044787B/en active Active
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| Publication number | Publication date |
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| CN106044787A (en) | 2016-10-26 |
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| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: No.46, ZHUJIAZHUANG commercial road, Rushankou Town, Rushan City, Weihai City, Shandong Province Patentee after: Rushan Dayang silica gel Co.,Ltd. Address before: ZHUJIAZHUANG, Rushankou Town, Rushan City, Weihai City, Shandong Province Patentee before: RUSHAN DAYANG SILICA GEL FACTORY |
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| CP03 | Change of name, title or address | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A preparation method of aerogel Effective date of registration: 20230816 Granted publication date: 20180612 Pledgee: Agricultural Bank of China Limited Rushan City Branch Pledgor: Rushan Dayang silica gel Co.,Ltd. Registration number: Y2023980052410 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |